The two novel conglomerates were obtained by crystallization of racemic (2'S,3aS,6aR)/(2'R,3aR,6aS) (glycoluril-1-yl)-3-methylbutanoic acid and (2'R,3aR,6aR)/(2'S,3aS,6aS) (4,6-dimethylglycoluril-1-yl)pentanoic acid synthesized by highly diastereoselective condensation of 4,5-dihydroxy- imidazolidin-2-ones with racemic ureido acids. The differences in the molecular geometry of synthesized racemates were studied by X-ray diffraction that showed them to crystallize as conglomerates in non-centrosymmetric space groups Pna21 and P212121, respectively 相似文献
Pd is one of the metals suitable for inducing low-temperature crystallization in Ge. However, it is not clear how residual Pd atoms are integrated into the Ge lattice. Therefore, time-differential γ–γ perturbed angular correlations (TDPAC) technique using the 100Pd(→100Rh) nuclear probe produced by recoil implantation has been applied to study the hyperfine interactions of this probe in single-crystalline undoped Ge. A Pd-vacancy complex aligned along the <111> crystallographic direction with a unique interaction frequency of 8.4(5) Mrad/s has been identified. This complex was measured to have a maximum relative fraction of about 76(4)% following annealing at 350 °C. Further annealing at higher temperatures reduced this fraction, possibly via dissociation of the complex. Calculations suggest dissociation energy of 1.94(5) eV for the complex. DFT calculations performed in this work are in reasonable good agreement with the experimental values for the electric-field gradient of the defect complex in Ge and Si for comparison. The calculations predict a split-vacancy configuration with the Pd on a bond-centred interstitial site having a nearest-neighbour semi-vacancy on both sides (V-PdBI-V) in Ge and Si. 相似文献
Pr-based bulk metallic amorphous (BMA) rods (Pr60Ni30Al10) and Al-based amorphous ribbons (Al87Ni10Pr3) have been prepared by using copper mould casting and single roller melt-spun techniques, respectively. Thermal parameters deduced from differential scanning calorimeter (DSC) indicate that the glass-forming ability (GFA) of Pr60Ni30Al10 BMA rod is far higher than that of Al87Ni10Pr3 ribbon. A comparative study about the differences in structure between the two kinds of glass-forming alloys, superheated viscosity and crystallization are also made. Compared with the amorphous alloy Al87Ni10Pr3, the BMA alloy Pr60Ni30Al10 shows high thermal stability and large viscosity, small diffusivity at the same superheated temperatures. The results of x-Ray diffraction (XRD) and transmission electron microscope (TEM) show the pronounced difference in structure between the two amorphous alloys. Together with crystallization results, the main structure compositions of the amorphous samples are confirmed. It seems that the higher the GFA, the more topological type clusters in the Pr-Ni-Al amorphous alloys, the GFAs of the present glass-forming alloys are closely related to their structures. 相似文献
This research aimed to reduce the variability on the data obtained from differential scanning calorimetric (DSC) analysis of the isothermal crystallization kinetics of cocoa butter.
To enable transformation of the DSC crystallization peak to a sigmoid crystallization curve, the DSC peak area has to be integrated. Usually, the start and end points of the crystallization peak are determined visually. The result of this visual determination appeared to be very much dependent on the operator, but also differed considerably when the same operator performed the integration several times. By proposing an objective calculation algorithm to determine the start and end points of integration, the variability caused by the operator during the integration procedure could be eliminated. Furthermore, sample preparation and the DSC heating protocol to melt the sample prior to crystallization were studied. Three heating protocols (65 °C for 15 min, 65 °C for 30 min and 80 °C for 15 min) were compared and it was shown that holding at 65 °C for 15 min was sufficient to eliminate any influence of sample history. Two different sample preparation procedures were compared and it appeared that a change in sample preparation procedure had a significant influence on the measured crystallization process. It is thus important to keep this method constant to eliminate the variability caused by it. 相似文献